The synthesization and characterization of amor-phous iron and stainless steel films have been the subject of this work. For this, various aspects of the carbide, nitride, oxide and boron-nitride formation and their stability were studied in detail to localize the parameter range of the metastable amorphous state in the given systems.
Intrigued by the predictions of Lee et al. [9], inert sputtering from a pre-combined Fe50C50 was used to synthesize the stoichiometric NaCl-type FeC phase via Magnetron-sputtering. Unfortunately, geometric effects of the target configuration, hysteresis effects and re-sputtering constitute severe problems to the deposition process. As a consequence of this, the Magnetron sputtering technique seems not to be suitable to synthesize the stoichiometric FeC phase, but the films exhibit carbon contents, which exceed the maximum solubility limits in known carbides. As a result, reactive sputtering of stainless steel - by using methane, nitrogen and oxygen as reactive gas - was performed to synthesize amorphous films or quasi metallic glasses based on conventional steels.
For carburized samples, following results were obtained. All carburized samples showed a broad appearance in the GIXRD patterns revealing the character of amorphous materials. The magnetic properties investigated by means of M¨ossbauer Spectroscopy and MOKE showed the formation of various phases and carbides at a sputtering temper-ature of 298 K. In addition a new amorphous and soft ferromagnetic phase was observed. For this phase, a median hyperfine field of< B >= 10.3 T with a width of σ = 6.1 T was obtained from the P(B) distribution of the M¨ossbauer analysis.
The soft ferromagnetic character was derived by MOKE, which revealed a coercive field of approximately 4 Oe. Furthermore, vacuum an-nealing of this phase showed the carbide reaction M7C3→M23C6→M6C.
To characterize the microstructure of the new amorphous and soft ferromagnetic phase, DSC, FIM, TEM and EXAFS experiments were carried
out for carburized samples.
DSC, FIM and TEM showed the quasi metallic glass behavior of these phase, but the microstruc-ture could only be explained by the EXAFS analysis, which revealed a disordered Ni3C phase.
The magnetism of this phase could be predicted by a LMTO model [119], the order of magnetism could be explained by a core-shell model, describing the nano-particles as consisting of a ferromagnetically core and a disordered surface shell [121, 122].
These experiments confirmed a pre-suggested model, which is based on thermodynamical and kinetic remarks of Lu et al. [13] and of Lux and Haubner [113]: the present Fe-based alloy is associated with the deep eutectic point of the Fe-C system. It is well known that compositions around the deep eutectic point are ideal for glass formation in many systems. As a result, glass formation is greatly favored thermodynamically.
Further, the minor addition of Mo could promote glass formation in the Fe-C system by suppressing the formation of the primary phase and hindering grain growth. Because of their limited solubility in Fe carbides, the molybdenum atoms must redistribute and long-range diffusion is required upon solidification. The introduction of a reactive sputtering gas - here the carbon from methane - additionally disturbs the nucleation process by establishing higher probabilities of coordination.
This leads to simultaneous rearrangement of different species of atoms, which suppresses the formation of competing ordered phases. As a consequence, phases outside the equilibrium can be formed like the disordered trigonal Ni3C phase.
To proof the transferability of this model to the p-block elements N and O, the reactive Magnetron-sputtering technique was used to deposit nitrided and oxidized sample. Indeed, both systems re-vealed the same amorphous and soft ferromagnetic phase.
As shown in Fig. 6.51, the FeN system can be understood as a perfect Gibbs system in the given parameter range, wherein the Fe3N phase
121
represents the minimum of that system. Combined with the shown tendency obtained for the reactive gas flow, any given phase - from amorphous to crystalline - can be reached for Magnetron-nitrided stainless steel films. In fact, amorphous and crystalline phases, such as the new amorphous and soft ferromagnetic and ZnS-type γ-(Fe,Cr,Ni)N phase, were observed.
In contrast, Fig. 6.61 exhibit the FeO system as a Gibbs plot of a multi-phase system, in which the transition from the amorphous state (domain I) to the crystalline phases (domain II - the formation of FeO, Fe2O3 oxides) is depicted. In contrast to the carburized and nitrided amorphous and soft ferromagnetic phase, M¨ossbauer Spectroscopy and RBS of the oxidized phase indicated the participation of Fe-oxides. As a consequence, the model for the amorphous state for carburized and nitrided samples can not be applied in the same form for oxidized samples.
According to He et al. [118] and Kodama et al. [135], NiFe2O4 cores surrounded by spin-glassy surface shells would satisfy the observed results.
This hypothesis has to be proven in upcoming EXAFS experiments.
Reconsidering all experiments, it is reasonable to assume, that the model mentioned above is transferable to all p-block elements.
As next step, the verifiability of the model con-cerning the synthesization mode was investigated.
Therefore, the PLD technique was chosen to synthesize high-carbon iron and stainless steel films. For this purpose, the STPLD technique was developed to enlarge the advantages of the PLD.
Until the introduction of STPLD, either precasted PLD targets had to chosen or complex rotating target systems were in use. Now, the material and area fraction of the STPLD inlay extend the number of processing parameters.
Whereas the magnetron sputtering technique failed, the in this work presented STPLD technique succeeded: by pre-combining an ARMCO target with an graphite inlay, the prediction of Lee et al. [9], that a NaCl-type FeC phase can be formed, could be confirmed. Films with 20 nm in thick-ness were directly deposited on TEM grids and immediately TEM analyzed. A Fe-C bond length of 0.229(3) nm and, thus, a lattice parameter of a0 = 0.458(6) nm was obtained. This is in good agreement with Lee’s predictions (bond length 0.236 nm and a0 = 0.473 nm). Unfortunately, the synthesization of stoichiometric FeC films failed, which could be originated in inter-diffusion with the a-SiO2 substrate [140] or by a thickness effect [141].
The STPLD of stainless steel - graphite targets lead to the formation of self-organized multilayer
films. Together with the solidification disturbance induced by Mo atoms, carbon diffuses through the metal matrix. Local carbon inhomogeneities were induced via the target scan process. This induces local diffusion gradients which leads to an self-organizing effect and which promotes the decomposition of carbon and stainless steel and assists multilayer formation plus the formation of superstructures. By increasing the ion energies by increasing the scan velocity, an additionally implantation of the target materials lead to a locally rearrangement which hinders the overall carbon diffusion in the matrix, but not complete.
As a consequence, the size of the superstructure is reduced. The ion implantation could lead to op-posing diffusion gradients in the nano-scale regime, which could lead again to a self-organization and the formation of multilayer by decomposing carbon and stainless steel.
The STPLD technique was also used, to synthesize Al/C and Ti/C multilayer. As a consequence, an exponential correlation between the layer thickness and the atomic number of the metallic component of the target was found.
Unfortunately, the growth mechanism is not fully understood and several experiments have to be carried out to find an empirical formula, which describes the multilayer thickness.
As next step, the inlay material was varied and boron-nitride was used. The boro-nitrided stainless steel film exhibit a verisimilar amorphous phase, which was observed in carburized, nitrided and ox-idized stainless steel films. The difference between these amorphous phases is found in magnetism.
Whereas the amorphous phase in magnetron and RPLD deposited exhibits two magnetic compo-nents and is soft ferromagnetic, the boro-nitrided amorphous phase exhibits only one magnetic component, which could be identified as FeB phase and the coercive field is by a factor of 10 higher.
This indicates, that the missing high-hyperfine field component in the M¨ossbauer spectra is attributed to a spin glassy phase containing Fe. As a result, harder magnetism is observed.
Surprisingly, the synthesization of SS/BN STPLD films only revealed a weak AMF, which could be due to the deposition of BN-droplets. These par-ticulates offer potentials, on which the adsorbents nucleate. As a consequence, multilayer growth is hindered.
Also RPLD films exhibit the amorphous and soft and ferromagnetic phase. With the aid of this process, the nucleation model was confirmed and further improved. Furthermore, STPLD and RPLD confirmed the independence of the nucleation model on the preparation mode of the films.
123
For comparison, the amorphization behavior of surface treated samples was investigated. There-fore, FEL experiments at the Jefferson lab were carried out, wherein the nitrogen incorporation was assisted by laser beam radiation.
FEL surface processing of stainless steel sam-ples lead to the formation of a well-crystallized γ-(Fe,Cr,Ni) surface layer. FEL treatment of AISI 310 improved the hardness. A film thickness of of t = 4.85(5) µm and Hf was derived to 2.64(3) GPa. For AISI 316, the film hardness was derived to Hf = 2.49(2) GPa; the layer thickness to 5.84(40)µm. Thus, the FEL revealed its most important advantage: an extremely fast treatment process which allows the formation of functional layers in the micron-scale. However, further experiments have to be done to localize the parameter range (overlap-parameter, laser energy, scan speed, chamber pressure etc.) to obtain amorphous surface layers.
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